CN106770783B - A kind of method that liquid-liquid micro-extraction closes 9 kinds of aromatic amines in phase chromatographic tandem mass spectrography detection cigarette mainstream flue gas - Google Patents

A kind of method that liquid-liquid micro-extraction closes 9 kinds of aromatic amines in phase chromatographic tandem mass spectrography detection cigarette mainstream flue gas Download PDF

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CN106770783B
CN106770783B CN201710012585.2A CN201710012585A CN106770783B CN 106770783 B CN106770783 B CN 106770783B CN 201710012585 A CN201710012585 A CN 201710012585A CN 106770783 B CN106770783 B CN 106770783B
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aromatic amines
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CN106770783A (en
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邓惠敏
杨飞
王颖
李中皓
边照阳
范子彦
刘珊珊
衡英英
唐纲岭
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NATIONAL TOBACCO QUALITY SUPERVISION TESTING CENTER
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N2030/022Column chromatography characterised by the kind of separation mechanism
    • G01N2030/027Liquid chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • G01N2030/062Preparation extracting sample from raw material

Abstract

A kind of method that liquid-liquid micro-extraction closes 9 kinds of aromatic amines in phase chromatographic tandem mass spectrography detection cigarette mainstream flue gas, it is characterized by: the aromatic amine of the release in main flume is trapped by cambridge filter first, internal standard is added, mechanical shaking extraction is carried out to the cambridge filter that suction obtains with aqueous hydrochloric acid solution, sodium hydrate aqueous solution is added, pH is adjusted to 12 ~ 13, a certain amount of extractant toluene is added, salting-out agents sodium chloride is shaked, upper toluene layer is taken out after centrifugation, to close phase chromatographic tandem mass spectrography (UPC2- MS/MS) fragrant amine content therein is analyzed, and quantified by internal standard method.The sample pre-treatments of this method are easy to operate, quick, and the analysis detection time is short, and the reproducible of method, the rate of recovery are high, analyze convenient for batch sample.

Description

A kind of liquid-liquid micro-extraction closes 9 in phase chromatographic tandem mass spectrography detection cigarette mainstream flue gas The method of kind aromatic amine
Technical field
The invention belongs to chemical analysis fields, and in particular to a kind of combined using liquid-liquid micro-extraction technology closes phase chromatographic tandem Mass spectrography (UPC2- MS/MS) to the quick quantitative analytic method of the burst size of 9 kinds of aromatic amines in cigarette mainstream flue gas.
Background technique
Aromatic amine refers to the amine with an armaticity substituent, and there is also some aromatic amines in cigarette smoke.2012 Food and drug administration (FDA) publication about in tobacco product and flue gas harmful substance and potentially harmful substance at Divide in list and clearly outlines to naphthalidine, 2- naphthylamines, 3- aminobphenyl, 4- aminobphenyl, o-aminoanisole, 2,6- diformazan The control and disclosure of base aniline and ortho-aminotoluene ingredient.
The detection method of aromatic amine chemicals mainly has gas chromatography, gas chromatography mass spectrometry, liquid phase color in flue gas Compose tandem mass spectrometry etc..And the relevant report for closing aromatic amine in phase chromatographic tandem mass spectrography detection main flume is had not seen at present. As a kind of emerging instrument detection technique, phase chromatographic mass spectrometry is closed with nontoxic, nonflammable and free from environmental pollution supercritical fluid CO2It is a kind of real green environmental protection technique as main mobile phase, and has many dash forward compared to liquid chromatogram and gas-chromatography Advantage out has separating degree and selectivity well for analogue, isomers, enantiomer and diastereoisomer.
Liquid-liquid micro-extraction is a kind of Sample Pretreatment Technique to grow up from 2006, can be considered liquid-liquid extraction solvent The treatment process of minimum.Currently, liquid-liquid micro-extraction technology is because it has the characteristics that easy, to extract thickening efficiency high, in water The analysis field of low pole substance is widely applied in phase.
The present invention is directed to the sample features according to cigarette smoke, using liquid-liquid micro-extraction pre-treating method, by closing phase color Compose tandem mass spectrometry in cigarette mainstream flue gas 9 kinds of aromatic amines (naphthalidine, 2- naphthylamines, 3- aminobphenyl, 4- aminobphenyl, O-aminoanisole, 2,6- dimethylaniline, ortho-aminotoluene, meta-aminotoluene, para-totuidine) analysis detection is carried out, simplify sample Pretreatment process shortens the analysis detection time, provides technology to the detection research work of aromatic amine harmful components in cigarette product It supports.
Summary of the invention
The object of the present invention is to provide 9 kinds of aromatic amines (naphthalidine, 2- naphthylamines, 3- amino connection in a kind of cigarette mainstream flue gas Benzene, 4- aminobphenyl, o-aminoanisole, 2,6- dimethylaniline, ortho-aminotoluene, meta-aminotoluene, para-totuidine) UPC2- MS/MS analysis method mainly carries out suction test to cigarette sample first, with the fragrance in cambridge filter trapping main flume Then amine is pre-processed using liquid-liquid micro-extraction pretreatment technology, finally use UPC2- MS/MS detects aromatic amine, And quantitative analysis is carried out by internal standard method.
The purpose of the present invention is achieved through the following technical solutions:
A kind of method that liquid-liquid micro-extraction closes 9 kinds of aromatic amines in phase chromatographic tandem mass spectrography detection cigarette mainstream flue gas, it is first The aromatic amine for first passing through the release in cambridge filter trapping main flume, is added internal standard, is obtained with aqueous hydrochloric acid solution to suction Cambridge filter carries out mechanical shaking extraction, and sodium hydrate aqueous solution is added by pH and is adjusted to 12 ~ 13, a certain amount of extractant first is added Benzene, salting-out agents sodium chloride are shaked, and upper toluene layer are taken out after centrifugation, to close phase chromatographic tandem mass spectrography (UPC2- MS/MS) Fragrant amine content therein is analyzed, and is quantified by internal standard method.Specific step is as follows:
(1) sample pre-treatments:
First Canadian depth suction mode (55 mL of pumping volume, 2 s of suction time, suction frequencies 30 s, 100% Blocking filtering ventilation hole) under, suction test is carried out to 10 reference cigarette samples using rotating disc type smoking machine, suction is obtained Cambridge filter is put into 100 mL plastic bottles, and 60 mL, 5% aqueous hydrochloric acid solution is added into bottle and 250 μ L concentration are 4.0 The mixing inner mark solution of mg/L, plastic bottle is placed on oscillator, extracts 30 min with the rate oscillation of 1000 r/min;To bottle 2 mL of extractant toluene is added to adjust pH to 12 ~ 13 in the middle sodium hydrate aqueous solution that 4.0 mol/L are added, and addition is saltoutd Then 2 g of agent sodium chloride is centrifuged 2 min with 10000 r/min, takes in vibrating 2 min on vortex mixed instrument with 2000 r/min Upper toluene layer out, be added to 2 mL include 50 mg N- propyl ethylenediamines, 50 mg C18,7.5 mg Graphons, 150 In the dispersive solid-phase extraction purification pipe of mg anhydrous magnesium sulfate, in vibrating 2 min on vortex mixed instrument with 2000 r/min, then 2 min, as sample prepare liquid are centrifuged with 10000 r/min;
(2) standard working solution is prepared: prepare include 9 kinds of aromatic amines and 6 kinds of deuterated interior target list mark stock solutions preparation, The preparation of 9 kinds of aromatic amines and the mixed mark stock solution of 6 kinds of deuterated interior targets and the preparation of series standard working solution;Detailed process is such as Under:
Single mark stock solution: the 9 kinds of aromatic amines and 6 kinds that mass concentration is 1 mg/mL are prepared respectively using methanol as solvent Deuterated interior target list mark stock solution;
Mixed mark stock solution: 200 μ L ortho-aminotoluenes, meta-aminotoluene, para-totuidine are pipetted respectively;50 μ L naphthalidines, 2- naphthalene Amine;20 μ L 2,6- dimethylanilines;Single mark stock solution of 10 μ L 3- aminobphenyls, 4- aminobphenyl, o-aminoanisole, 10 mL are settled to toluene, obtain the mixing stock solution of 9 kinds of aromatic amines;The deuterated interior target list mark of 6 kinds of 50 μ L is pipetted respectively Stock solution is settled to 25 mL with toluene, obtains 6 kinds of deuterated interior targets that mass concentration is 4 mg/mL and mixes stock solution;
Series standard working solution: accurately pipette respectively 0.01 mL, 0.02 mL, 0.05 mL, 0.1 mL, 0.2 mL, The mixing stock solution of 9 kinds of aromatic amines of 0.3 mL is separately added into 6 kinds of deuterated interior target mixing stock solutions of 50 μ L, dilute with toluene It releases and is settled to 2 mL, obtain series standard working solution.
(3) UPC2- MS/MS measurement:
Draw prepared series standard working solution injection UPC2- MS/MS, with standard series peak area and internal standard peak face Its quality of the comparison of product establishes equation of linear regression, is measured to sample prepare liquid, measures the peak area of each target aromatic amine The ratio between with interior target peak area, equation of linear regression is substituted into, the content of 9 kinds of aromatic amines in sample is respectively obtained.
UPC2- MS/MS analysis condition
Chromatographic condition: chromatographic column selects HSS C18 chromatographic column, 1.7 mm;Column temperature: 60 DEG C;Sample volume: 2 mL;Cosolvent: Methanol;Flow velocity: 2 mL/min;Compensate solvent: the methanol of 0.1% formic acid;Flow velocity: 0.2 mL/min;Gradient is as shown in table 1:
Mass Spectrometry Conditions: ion source: electrospray ionisation source (ESI), temperature: 150 DEG C;Capillary voltage: 3.0 kV;Remove solvent Temperature degree: 300 DEG C;Go solvent stream fast: 800 L/h;Blowback gas velocity: 50 L/h;Multiple-reaction monitoring pattern (MRM), in detail Parameter is shown in Table 2.
The present invention has the effect that
(1) this method first passage liquid-liquid micro-extraction pre-treating method establishes 9 kinds of fragrance in a kind of cigarette mainstream flue gas The mass spectrographic rapid assay methods of conjunction phase chromatographic tandem of amine.Mainly according to cigarette smoke sample the characteristics of, to liquid-liquid micro-extraction Extraction solvent, salting-out agents of pre-treating method etc. have carried out selection and optimization, and to the chromatographic column for influencing chromatographic separation condition Selection, the selection of cosolvent, flow velocity and system back pressure are optimized.
(2) sample pretreatment process of this method and conjunction phase chromatographic tandem Mass Spectrometer Method process are simple, quick, save significantly Analysis time has been saved, has been analyzed convenient for batch sample.
(3) this method is reproducible, the detection of 9 kinds of aromatic amine burst sizes suitable for cigarette mainstream flue gas.
Detailed description of the invention:
Fig. 1: measuring method flow chart of the present invention.
Fig. 2: the selection of Extraction solvent.
Fig. 3: the selection of salting-out agents.
Fig. 4: standard working solution total ion current figure.
Specific embodiment
Present invention combination example is described further, but is not the limitation present invention.
Example 1:
(1) instrument and reagent:
It closes phase chromatographic tandem mass spectrograph (Waters, US);RM-200A rotating disc type smoking machine (German Borgwaldt Company);Labnet VX-200 vortex mixed instrument (Labnet company of the U.S.);Sigma 3-30K high speed freezing centrifuge (Germany Sigma company);Milli-Q ultrapure water system (Millipore company of the U.S.).
Ortho-aminotoluene (o-TOL), meta-aminotoluene (m-TOL), para-totuidine (p-TOL), 2,6- dimethylaniline (2,6- DMA), o-aminoanisole (o-ASD), naphthalidine (1-NA), 2- naphthylamines (2-NA), 3- aminobphenyl (3-ABP), 4- amino connection Benzene (4-ABP), D9- ortho-aminotoluene (o-TOL-d9), D7- o-aminoanisole (o-ASD-d7), D7-1- naphthylamines (1-NA-d7), D7-2- naphthylamines (2-NA-d7), D11-2,6- dimethylaniline (2,6-DMA-d11), D9-4- aminobphenyl (4-ABP-d9) (moral Dr. Ehrensorfer company of state);Toluene, n-hexane, hexamethylene (chromatographically pure, J. T. Baker company of the U.S.), hydroxide Sodium, sodium chloride, sodium sulphate (analyzing pure, Tianjin north Reagent Company), the dispersive solid-phase extraction of 2 mL purify kit (50 mg N- propyl ethylenediamine, 50 mg C18,7.5 mg Graphons, 150 mg anhydrous magnesium sulfates) (Agilent company of the U.S.); 3R4F reference cigarette sample (Kentucky, United States university).
(2) sample pre-treatments:
First Canadian depth suction mode (55 mL of pumping volume, 2 s of suction time, suction frequencies 30 s, 100% Blocking filtering ventilation hole) under, suction test is carried out to reference cigarette sample (10) using rotating disc type smoking machine.Suction is obtained Cambridge filter be put into 100 mL plastic bottles, 60 mL, 5% aqueous hydrochloric acid solution is added into bottle and 250 μ L concentration are The mixing inner mark solution of 4.0 mg/L, plastic bottle is placed on oscillator, extracts 30 min with the rate oscillation of 1000 r/min. The sodium hydrate aqueous solution of 4.0 mol/L is added into bottle to adjust pH to 12 ~ 13,2 mL of extractant is added, addition is saltoutd Then 2 g of agent sodium chloride is centrifuged 2 min in vibrating 2 min on vortex mixed instrument with 2000 r/min with 10000 r/min.It takes Out upper layer extract oxidant layer, be added to 2 mL dispersive solid-phase extraction purification pipe (50 mg N- propyl ethylenediamines, 50 mg C18, 7.5 mg Graphons, 150 mg anhydrous magnesium sulfates) in, in vibrating 2 min on vortex mixed instrument with 2000 r/min, so 2 mi are centrifuged with 10000 r/min afterwards, supernatant is taken to wait for UPC2- MS/MS analysis.
Wherein respectively using toluene, n-hexane and hexamethylene as extractant, the selection of extractant is optimized, is tied Fruit is as shown in Figure 2.The result shows that the extraction efficiency highest of toluene.In addition, the selection to salting-out agents is also optimized.Such as Fig. 3 It is shown, the results showed that salting-out agents are added and help to improve extraction efficiency, because the difference of sodium chloride and sodium sulphate is little, final choice Sodium chloride is as salting-out agents.
(3) preparation of standard working solution
The preparation of standard working solution mainly includes the preparation of 9 kinds of aromatic amines and 6 kinds of deuterated interior target list mark stock solutions, 9 The preparation of kind aromatic amine and the mixed mark stock solution of 6 kinds of deuterated interior targets and the preparation of series standard working solution, were specifically prepared Journey is as previously described, is not repeated herein.
(4) UPC2- MS/MS analysis
9 kinds of aromatic amines of influence and 6 kinds of deuterated interior target mass spectrometry parameters are optimized first.Then impact analysis is imitated The experiment condition of fruit has carried out system optimization, including chromatographic column, cosolvent, flow velocity.The result shows that separating effect on a cl 8 column Preferably, 9 kinds of aromatic amine whole appearances, and can obtain when being 2.0 mL/min using methanol as cosolvent, system flow rate best Separating degree.The total ion current figure for obtaining standard solution in optimal conditions is as shown in Figure 4.
(5) result is analyzed
The standard working solution of 6 kinds of concentration is subjected to UPC2- MS/MS analysis, with object and interior target chromatographic peak area The concentration for comparing aromatic amine carries out regression analysis, obtains standard curve and its regression equation, related coefficient, this law linear relationship is good Good, the results are shown in Table 3.
Suction test is carried out to 3R4F reference cigarette, UPC is carried out to aromatic amine burst size therein2- MS/MS analysis is surveyed It is fixed.In addition, the standard solution of three kinds of various concentrations is added on the cambridge filter for being loaded with smoke's total particulate matter, calculates mark-on and return Yield the results are shown in Table 4.It can be seen that except the rate of recovery of 6-DMA is lower, the range of the rate of recovery of other 8 kinds of aromatic amines is equal in addition to 2 Between 66%~130%.The relative standard deviation and the rate of recovery of 2,6-DMA measurement results are lower, this may be due to 2, 6-DMA volatility is relatively strong caused, therefore should analyze as early as possible after sample pretreatment.
In addition, the measurement result of this method and the measurement result of traditional existing national standard method are compared, as a result As shown in table 5, it is seen that in addition to the measurement result of 3-ABP and 4-ABP has different, for remaining 7 kinds of aromatic amine this method with The consistency of conventional method measurement result is preferable.Since the pretreatment process based on liquid-liquid micro-extraction of this method is simple, and adopt With novel, environmental protection, phase chromatographic tandem mass spectrography is quickly closed, thus provides fragrance in a kind of fast and accurately main flume The new method of amine measurement.

Claims (3)

1. a kind of method that liquid-liquid micro-extraction closes 9 kinds of aromatic amines in phase chromatographic tandem mass spectrography detection cigarette mainstream flue gas, described 9 Kind aromatic amine specifically: naphthalidine, 2- naphthylamines, 3- aminobphenyl, 4- aminobphenyl, o-aminoanisole, 2,6- dimethyl benzene Amine, ortho-aminotoluene, meta-aminotoluene, para-totuidine, it is characterised in that: trap the release in main flume by cambridge filter first Aromatic amine, internal standard is added, mechanical shaking extraction is carried out to the obtained cambridge filter of suction with aqueous hydrochloric acid solution, sodium hydroxide water is added PH is adjusted to 12 ~ 13 by solution, a certain amount of extractant toluene is added, salting-out agents sodium chloride is shaked, and is taken out after centrifugation Upper toluene layer, to close phase chromatographic tandem mass spectrography UPC2- MS/MS analyzes fragrant amine content therein, and by interior Mark method is quantified;Specific step is as follows:
(1) sample pre-treatments:
First under Canadian depth suction mode, suction survey is carried out to 10 reference cigarette samples using rotating disc type smoking machine The obtained cambridge filter of suction is put into 100 mL plastic bottles by examination, be added into bottle 60 mL, 5% aqueous hydrochloric acid solution and 250 μ L concentration are the mixing inner mark solution of 4.0 mg/L, plastic bottle are placed on oscillator, with the rate oscillation of 1000 r/min Extract 30 min;The sodium hydrate aqueous solution of 4.0 mol/L is added into bottle to adjust pH to 12 ~ 13, extractant first is added 2 g of salting-out agents sodium chloride is added in 2 mL of benzene, in vibrating 2 min on vortex mixed instrument with 2000 r/min, then with 10000 R/min is centrifuged 2 min, takes out upper toluene layer, and being added to 2 mL includes 50 mg N- propyl ethylenediamines, 50 mg C18, and 7.5 Mg Graphon, 150 mg anhydrous magnesium sulfates dispersive solid-phase extraction purification pipe in, on vortex mixed instrument with 2000 r/ Min vibrates 2 min, is then centrifuged 2 min, as sample prepare liquid with 10000 r/min;
(2) standard working solution is prepared: preparation includes the preparation of 9 kinds of aromatic amines and 6 kinds of deuterated interior target list mark stock solutions, 9 kinds The preparation of aromatic amine and the mixed mark stock solution of 6 kinds of deuterated interior targets and the preparation of series standard working solution;
(3) UPC2- MS/MS measurement:
Draw prepared series standard working solution injection UPC2- MS/MS, with standard series peak area and internal standard peak area it Compare its quality and establish equation of linear regression, sample prepare liquid is measured, measure the peak area of each target aromatic amine with it is interior The ratio between target peak area substitutes into equation of linear regression, respectively obtains the content of 9 kinds of aromatic amines in sample;
UPC2- MS/MS analysis condition
Chromatographic condition: chromatographic column selects HSS C18 chromatographic column, 1.7 mm;Column temperature: 60 DEG C;Sample volume: 2 mL;Cosolvent: first Alcohol;Flow velocity: 2 mL/min;Compensate solvent: the methanol of 0.1% formic acid;Flow velocity: 0.2 mL/min;Gradient is as shown in the table:
1. gradient of table
Time (min) CO2(%) Methanol (%) 0 99 1 0.5 99 1 2.5 96 4 3.2 97 3 3.5 70 30 5 99 1
Mass Spectrometry Conditions: ion source: electrospray ionisation source (ESI), temperature: 150 DEG C;Capillary voltage: 3.0 kV;Remove solvent temperature Degree: 300 DEG C;Go solvent stream fast: 800 L/h;Blowback gas velocity: 50 L/h;Multiple-reaction monitoring pattern (MRM).
2. method according to claim 1, it is characterised in that: Canadian depth suction mode is specific in step (1) Condition are as follows: 55 mL of pumping volume, 2 s of suction time, 30 s of suction frequencies, 100% blocking filtering ventilation hole.
3. method according to claim 1, it is characterised in that: detailed process is as follows for standard working solution preparation:
Single mark stock solution: preparing 9 kinds of aromatic amines that mass concentration is 1 mg/mL using methanol as solvent respectively and 6 kinds deuterated Interior target list mark stock solution;
Mixed mark stock solution: 200 μ L ortho-aminotoluenes, meta-aminotoluene, para-totuidine are pipetted respectively;50 μ L naphthalidines, 2- naphthylamines; 20 μ L 2,6- dimethylanilines;Single mark stock solution of 10 μ L 3- aminobphenyls, 4- aminobphenyl, o-aminoanisole, with Toluene is settled to 10 mL, obtains the mixing stock solution of 9 kinds of aromatic amines;The deuterated interior target list mark deposit of 6 kinds of 50 μ L is pipetted respectively Liquid is settled to 25 mL with toluene, obtains 6 kinds of deuterated interior targets that mass concentration is 4 mg/mL and mixes stock solution;
Series standard working solution: 0.01 mL, 0.02 mL, 0.05 mL, 0.1 mL, 0.2 mL, 0.3 mL are accurately pipetted respectively 9 kinds of aromatic amines mixing stock solution, 6 kinds of 50 μ L deuterated interior targets mixing stock solutions are separately added into, with dilution with toluene constant volume To 2 mL, series standard working solution is obtained.
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